A method for improving the color depth and glossiness of black cellulose fibers

Abstract

The present invention provides a method for improving the color depth and glossiness of black cellulose fiber, the method comprising the preparation of a carbon nanotube dispersion system, the preparation of a mixed black slurry dispersion system, the preparation of a blended spinning solution, spinning and post-treatment; the post-treatment comprises reactive dye finishing and cationic modified color fixation. The colored cellulose fiber prepared by the present invention has good color fastness. Compared with the cellulose fiber colored by the single solution, the color depth and glossiness are greatly improved, the color fastness to soaping is 4.0~5.0, and the color fastness to rubbing is 4.0~5.0; compared with the cellulose fiber colored by the single solution, the color depth and glossiness are greatly improved. The color depth F / S value of the black cellulose fiber prepared by the present invention is ≥30.125, and the glossiness of the prepared black cellulose fiber is ≥22.57%.

Description

Technical Field

[0001] The invention relates to a method for improving the color depth and glossiness of black cellulose fibers, and belongs to the field of cellulose fiber manufacturing. Background Art

[0002] Cellulose fiber has the characteristics of good moisture absorption, comfortable wearing and excellent spinnability. It is often blended and interwoven with cotton, wool or various synthetic fibers. Therefore, cellulose fiber has been widely used in various types of clothing and decorative textiles. With the continuous improvement of people's living standards and the increasing attention to environmental protection, people's demand for high-end fabrics is increasing, and the requirements for their raw materials are becoming more and more stringent. Among them, colored cellulose fiber is becoming more and more important, and bright and pure colored cellulose fiber is more popular with customers, which is the market development trend of colored cellulose fiber.

[0003] One of the main methods is to prepare colored cellulose fibers by adding color paste to spinning solution. The colored cellulose fibers prepared by this method have high color fastness, but are easily affected by the color of the raw materials, and the cleaning process of the system is more difficult. In addition, its glossiness and color depth are far inferior to those of colored cellulose fibers prepared by subsequent dyeing.

[0004] In view of this, in view of the problems existing in the production process of pre-spinning injection-dyed cellulose fibers, how to improve the color depth and glossiness of liquid-dyed cellulose fibers and prepare high-quality colored cellulose fibers is a problem that the industry needs to solve. Summary of the invention

[0005] The technical problem to be solved by the present invention is to provide a method for improving the color depth and glossiness of black cellulose fibers in view of the above technical deficiencies and research status, so as to achieve the following invention purposes:

[0006] The black cellulose fiber is prepared by solution dyeing method to improve its color depth and glossiness.

[0007] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0008] A method for improving the color depth and glossiness of black cellulose fibers, the method comprising the preparation of a carbon nanotube dispersion system, the preparation of a mixed black slurry dispersion system, the preparation of a blended spinning solution, spinning and post-treatment; the post-treatment comprises reactive dye finishing and cationic modified color fixation.

[0009] The specific steps include:

[0010] 1. Preparation of carbon nanotube dispersion system

[0011] A certain amount of carbon nanotubes was weighed and added to the black color paste purchased from Suzhou Shiming Technology Co., Ltd., and ultrasonically dispersed at room temperature with an ultrasonic frequency of 7×10 6 ~2×10 9 Hz, treatment time 25~60min, to obtain a carbon nanotube dispersion system.

[0012] The mass fraction of black pigment in the black color paste slurry is 18-25%;

[0013] The mass ratio of the carbon nanotubes to the black pigment is 1:18-22. The carbon nanotubes have a purity of ≥60%, preferably 60-65%, a length of 1-3 microns, and an outer diameter of 2-4 nm.

[0014] 2. Preparation of mixed black slurry dispersion system

[0015] The carbon nanotube dispersion system prepared above was mixed with the black color paste slurry (black pigment mass fraction of 20%) produced by Suzhou Shiming Technology Co., Ltd. in a mass ratio of 1:1, and a pore-forming agent was added, and then deionized water was added for dilution to obtain a mixed black slurry dispersion system.

[0016] The total mass fraction of the black pigment and the carbon nanotubes in the mixed black slurry dispersion system is 10%, and the mass fraction of the pore former is 5%. The pore former is one of carbonate or bicarbonate, preferably sodium carbonate or sodium bicarbonate.

[0017] 3. Preparation of blended spinning solution

[0018] Cellulose pulp is used as raw material, and a cellulose spinning solution is obtained through a subsequent known viscose preparation process. The mixed black slurry dispersion system prepared above is added according to the effective ingredients, which accounts for a certain proportion of the type A cellulose content in the cellulose spinning solution, to prepare a blended spinning solution.

[0019] The cellulose spinning stock solution contains 8.5-10.0% cellulose A, 4.5-6.0% sodium hydroxide and a viscosity of 35-60s.

[0020] The total mass of the black pigment and the carbon nanotubes in the mixed black slurry dispersion system accounts for 3.5% to 5.0% of the mass of the methyl cellulose content, and the mass proportion of the corresponding pore former is 1.75% to 2.5%.

[0021] 4. Spinning and post-processing

[0022] The blended spinning stock solution is passed through a well-adjusted specific coagulation bath, or a special-shaped spinneret hole such as a flat or cross-shaped spinneret hole is used for spinning. The primary filament bundle is drawn to obtain a formed filament bundle. The obtained filament bundle is cut, evenly laid into a net, deacidified, first washed, desulfurized, second washed, finished with reactive dyes, cationic modified color fixation, third washed, acid washed, and refined in an oil bath, as well as pressed and dried to obtain black cellulose fibers with significantly improved color fastness and glossiness.

[0023] The surface of the prepared black cellulose fiber is made smoother by using an adjusted coagulation bath spinning process or a special-section spinneret forming process, thereby increasing the reflectivity and glossiness; the addition of a pore-forming agent increases the surface and internal pore structure and specific surface area of ​​the prepared cellulose fiber, thereby improving the adsorption capacity for black reactive dyes and cationic modifiers, thereby further improving the color depth of the fiber.

[0024] The coagulation bath comprises 90-110 g / L sulfuric acid and 280-295 g / L sodium sulfate, and the temperature is 45-50°C. When a special-shaped spinneret hole is selected, the coagulation bath composition is 90-110 g / L sulfuric acid, 15-20 g / L zinc sulfate, 280-295 g / L sodium sulfate, and the temperature is 45-50°C.

[0025] The uniform web laying method is to lay the web with a web laying liquid, the web laying liquid is water, the temperature is ≥97°C, preferably 97-99.2°C, and the web laying is carried out by agitation with high temperature water, and the high temperature web laying allows carbon disulfide to be evaporated as much as possible to reduce the sulfide content in the fiber. The thickness of the laid cotton layer is 5-12mm.

[0026] Deionized water is used for the deacidification, the first water washing, the second water washing and the third water washing at a temperature of 60-80° C. The processing time is controlled according to the chain speed, and the processing time for each process is 2.5-5 minutes.

[0027] The desulfurization bath material is sodium hydroxide or sodium sulfide, the concentration is 3.5-5.0 g / L, the temperature is 75-90° C., and the desulfurization time is 2.5-6 min.

[0028] The reactive dye finishing is carried out in a dye liquor containing a black reactive dye at a temperature of 60-80° C. for a processing time of 8-12 minutes.

[0029] The black reactive dye is reactive black BES, purchased from Shandong Hongfu Chemical Co., Ltd.;

[0030] The dye liquor containing black reactive dye has a mass concentration of 3.0-5.0% and a pH value of 6.5-7.5;

[0031] The cationic modification and color fixation are carried out in a cationic modification solution for 5 to 10 minutes;

[0032] The concentration of the cationic modifier in the cationic modified liquid is 30-50 g / L, and the pH value is 8-10;

[0033] The cationic modifier is one of GW cationic modifier, RC cationic modifier or cationic polyacrylamide, purchased from Qingdao Dayin Chemical Co., Ltd.

[0034] Cationic modifiers are used to fix reactive dyes and modify black cellulose fibers to enhance their color absorption ability.

[0035] The pickling process uses a weak acid solution to treat the fiber for 2.5 to 5 minutes, preferably acetic acid or lactic acid, with a concentration of 6 to 10 g / L and a temperature of 40 to 60° C. The weak acid reacts with metals, ash, etc. on the fiber to improve the cleanliness of the fiber, thereby improving the fiber gloss.

[0036] The temperature of the oil bath is 45-65° C., the concentration is 4-9 g / L, the pH is 7.0-9.0, and the treatment time is 2.5-5 min.

[0037] The moisture content of the fiber after being squeezed by the high-pressure roller is 50-70%.

[0038] The drying is performed by steam drying, the drying steam pressure is 0.50-0.60 MPa, the temperature is 100-120° C., and the drying time is 25-40 min.

[0039] The colored cellulose fiber prepared by this method has good color fastness, with a color fastness to washing of 4.0~5.0 (GB / T 3921 "Textiles - Tests for Color Fastness - Color Fastness to Washing") and a color fastness to rubbing of 4.0~5.0 (GB / T 3920 "Textiles - Tests for Color Fastness - Color Fastness to Rubbing"); compared with cellulose fibers dyed with a single solution, the color depth and glossiness are greatly improved. The color depth F / S value of the black cellulose fiber prepared by the invention is ≥30.125, which is at least 6.75% higher than that of the solution-dyed cellulose fiber prepared by the same amount of black pigment added; the glossiness of the black cellulose fiber is ≥22.57% (GB / T 8686-1988 "Fabric Gloss Test Method" stipulates that 3 samples of 100 mm×100 mm are cut from each fabric, and the test is carried out using a YG 814 fabric gloss meter, and the average value is taken), which is at least 8.55% higher than that of the solution-dyed cellulose fiber prepared by the same amount of black pigment added; and due to the use of carbon nanotubes, it has a reinforcing effect, so that its dry breaking strength is increased by 6.62%.

[0040] Compared with the prior art, the present invention has the following beneficial effects:

[0041] 1. The present invention provides a method for improving the color depth and glossiness of black colored cellulose fibers. The method is carried out in the existing cellulose fiber production process, and the process is simple and easy to implement.

[0042] 2. The improvement of glossiness is mainly achieved in the following three aspects: by adjusting the cellulose fiber molding process, changing the morphological structure of black cellulose fibers and changing their reflection of light to improve the fiber gloss; the application of carbon nanotubes can also increase the fiber gloss; adding weak acid treatment during the refining process to reduce the presence of ash and further improve the fiber gloss.

[0043] 3. By adding pore-forming agents, more holes are created on the fiber surface and inside, increasing the specific surface area of ​​cellulose fibers. Subsequent adjustments to the cellulose fiber refining process, addition of reactive dye finishing, cationic modification and color fixation, etc., can jointly improve the color depth of the fibers.

[0044] 4. The colored cellulose fiber prepared by this method has good color fastness, and the color depth and glossiness are greatly improved compared with the single solution-dyed cellulose fiber. The color fastness to soaping is 4.0~5.0, and the color fastness to rubbing is 4.0~5.0; compared with the single solution-dyed cellulose fiber, the color depth and glossiness are greatly improved. The color depth F / S value of the black cellulose fiber prepared by this invention is ≥30.125, which is at least 6.75% higher than the solution-dyed cellulose fiber prepared by the same amount of black pigment added; the glossiness of the black cellulose fiber is ≥22.57%, which is at least 8.55% higher than the solution-dyed cellulose fiber prepared by the same amount of black pigment added. DETAILED DESCRIPTION

[0045] The preferred embodiments of the present invention are described below. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.

[0046] Embodiment 1:

[0047] A method for improving the color depth and glossiness of black cellulose fibers, mainly comprising the following steps:

[0048] 1. Preparation of carbon nanotube dispersion system

[0049] A certain amount of carbon nanotubes was weighed and added to the black color paste (mass fraction of black pigment was 20%) purchased from Suzhou Shiming Technology Co., Ltd., and ultrasonic dispersion was performed at room temperature with an ultrasonic frequency of 7×10 6 Hz, treatment time 60min, to obtain a carbon nanotube dispersion system.

[0050] The mass ratio of the carbon nanotubes to the black pigment is 1:20;

[0051] The carbon nanotubes have a purity of 65%, a length of 1 to 3 micrometers, and an outer diameter of 2 to 4 nm.

[0052] 2. Preparation of mixed black slurry dispersion system

[0053] The carbon nanotube dispersion system prepared above was mixed with the black color paste slurry (black pigment mass fraction of 20%) produced by Suzhou Shiming Technology Co., Ltd. in a mass ratio of 1:1, and a pore-forming agent was added, and then deionized water was added for dilution to obtain a mixed black slurry dispersion system.

[0054] The total mass fraction of the black pigment and the carbon nanotubes in the mixed black slurry dispersion system is 10%, the mass fraction of the pore former is 5%, and the pore former is sodium carbonate.

[0055] 3. Preparation of blended spinning solution

[0056] Cellulose pulp is used as raw material, and a cellulose spinning solution is obtained through a subsequent known viscose preparation process. The mixed black slurry dispersion system prepared above is added according to the effective ingredients, which accounts for a certain proportion of the type A cellulose content in the cellulose spinning solution, to prepare a blended spinning solution.

[0057] The cellulose spinning stock solution contains 8.5% cellulose alpha, 4.5% sodium hydroxide and a viscosity of 35s.

[0058] The mass ratio of the total mass of the black pigment and the carbon nanotubes in the mixed black slurry dispersion system to the mass ratio of the methyl cellulose content is 3.5%.

[0059] 4. Spinning and post-processing

[0060] The blended spinning solution is spun through an adjusted coagulation bath (using a conventional circular spinneret), and the primary filament bundle is drawn to obtain a formed filament bundle. The obtained filament bundle is cut, evenly laid into a web, deacidified, first washed, desulfurized, second washed, finished with reactive dyes, cationic modified color fixation, third washed, acid washed, refined in an oil bath, pressed, and dried to obtain black cellulose fibers with significantly improved color fastness and glossiness.

[0061] The coagulation bath includes 90 g / L sulfuric acid and 280 g / L sodium sulfate, and the temperature is 50°C.

[0062] The uniform web laying method is to form a web using a web laying liquid, the web laying liquid is water, the temperature is 97°C, and the web laying is carried out by agitation using high temperature water. The high temperature web laying allows carbon disulfide to be evaporated as much as possible, and the thickness of the laid cotton layer is 5 mm.

[0063] Deionized water is used for the deacidification, first water washing, second water washing and third water washing at a temperature of 60° C. The processing time is controlled according to the chain network speed, and the processing time for each process is 5 minutes.

[0064] The desulfurization bath material is sodium hydroxide, the concentration is 3.5 g / L, the temperature is 90° C., and the desulfurization time is 2.5 min.

[0065] The reactive dye finishing is to finish the cut short fibers in a dye solution containing a black reactive dye at a temperature of 60° C. for 12 minutes;

[0066] The black reactive dye is reactive black BES, purchased from Shandong Hongfu Chemical Co., Ltd.;

[0067] The dye liquor containing black reactive dye has a mass concentration of 3.0% and a pH value of 6.5;

[0068] The cationic modification and color fixation is to treat the cut short fibers in a cationic modification solution for 10 minutes;

[0069] The concentration of the cationic modifier in the cationic modified solution is 30 g / L, and the pH value is 8;

[0070] The cationic modifier is GW cationic modifier, purchased from Qingdao Dayin Chemical Co., Ltd.;

[0071] The pickling is carried out using an acetic acid solution for 5 minutes, the concentration of the acetic acid solution is 6 g / L, and the temperature is 60°C.

[0072] The temperature of the oil bath was 45° C., the concentration was 9 g / L, the pH was 7.0, and the treatment time was 2.5 min.

[0073] The moisture content of the fiber after the pressing is 50% after the high-pressure pressing roller.

[0074] The drying is performed by steam drying, the drying steam pressure is 0.50 MPa, the temperature is 100° C., and the drying time is 40 min.

[0075] The colored cellulose fiber prepared by this method has good color fastness, and the color depth and glossiness are greatly improved compared with the single solution-dyed cellulose fiber. The black cellulose fiber has a soap-washing color fastness of 4.0, a rubbing color fastness of 4.0, a color depth F / S value of 30.125, and a glossiness of 22.57%, which are 6.75% and 8.55% higher than the solution-dyed cellulose fiber prepared with the same amount of black pigment added, respectively.

[0076] Embodiment 2:

[0077] A method for improving the color depth and glossiness of black cellulose fibers, mainly comprising the following steps:

[0078] 1. Preparation of carbon nanotube dispersion system

[0079] A certain amount of carbon nanotubes was weighed and added to the black color paste (mass fraction of black pigment was 20%) purchased from Suzhou Shiming Technology Co., Ltd., and ultrasonic dispersion was performed at room temperature with an ultrasonic frequency of 3×10 8 Hz, treatment time 40min, to obtain a carbon nanotube dispersion system.

[0080] The mass ratio of the carbon nanotubes to the black pigment is 1:20;

[0081] The carbon nanotubes have a purity of 60%, a length of 1 to 3 micrometers, and an outer diameter of 2 to 4 nm.

[0082] 2. Preparation of mixed black slurry dispersion system

[0083] The carbon nanotube dispersion system prepared above was mixed with the black color paste slurry (black pigment mass fraction of 20%) produced by Suzhou Shiming Technology Co., Ltd. in a mass ratio of 1:1, and a pore-forming agent was added, and then deionized water was added for dilution to obtain a mixed black slurry dispersion system.

[0084] The total mass fraction of the black pigment and the carbon nanotubes in the mixed black slurry dispersion system is 10%, the mass fraction of the pore former is 5%, and the pore former is sodium carbonate.

[0085] 3. Preparation of blended spinning solution

[0086] Cellulose pulp is used as raw material, and a cellulose spinning solution is obtained through a subsequent known viscose preparation process. The mixed black slurry dispersion system prepared above is added according to the effective ingredients, which accounts for a certain proportion of the type A cellulose content in the cellulose spinning solution, to prepare a blended spinning solution.

[0087] The cellulose spinning stock solution contains 9.2% cellulose alpha, 5.5% sodium hydroxide and a viscosity of 51s.

[0088] The mass ratio of the total mass of the black pigment and the carbon nanotubes in the mixed black slurry dispersion system to the mass ratio of the methyl cellulose content is 4.5%.

[0089] 4. Spinning and post-processing

[0090] The blended spinning solution is spun by changing the structure of the spinneret hole (flat spinneret hole, aspect ratio of 5:1), and the primary filament bundle is drawn to obtain a formed filament bundle. The obtained filament bundle is cut, evenly laid into a net, deacidified, first washed, desulfurized, second washed, finished with reactive dyes, cationic modified color fixation, third washed, acid washed, refined in oil bath and other scouring baths, pressed, and dried to obtain black cellulose fibers with significantly improved color fastness and glossiness.

[0091] The coagulation bath composition is 90 g / L sulfuric acid, 15 g / L zinc sulfate, 280 g / L sodium sulfate, and the temperature is 50°C.

[0092] The uniform web laying method is to form a web using a web laying liquid, the web laying liquid is water, the temperature is 98°C, and the web laying is carried out by agitation using high temperature water. The high temperature web laying allows carbon disulfide to be evaporated as much as possible, and the thickness of the laid cotton layer is 10 mm.

[0093] The deacidification, first water washing, second water washing and third water washing all use deionized water at a temperature of 75° C. The processing time is controlled according to the chain network speed, and the processing time for each process is 3.5 minutes.

[0094] The desulfurization bath material is sodium sulfide, the concentration is 4.2 g / L, the temperature is 83° C., and the desulfurization time is 4 minutes.

[0095] The reactive dye finishing is to finish the cut short fibers in a dye solution containing a black reactive dye at a temperature of 72° C. for 10 minutes.

[0096] The black reactive dye is reactive black BES, purchased from Shandong Hongfu Chemical Co., Ltd.;

[0097] The dye solution containing black reactive dye has a mass concentration of 4.1% and a pH value of 7.0;

[0098] The cationic modification and color fixation is to treat the cut short fibers in a cationic modification solution for 8 minutes;

[0099] The concentration of the cationic modifier in the cationic modified solution is 41 g / L, and the pH value is 9.2;

[0100] The cationic modifier is RC cationic modifier, purchased from Qingdao Dayin Chemical Co., Ltd.

[0101] The pickling is carried out using an acetic acid solution with a concentration of 8.5 g / L and a temperature of 55° C. for 3.5 min;

[0102] The temperature of the oil bath was 56° C., the concentration was 7.5 g / L, the pH was 8.0, and the treatment time was 4 min.

[0103] The moisture content of the fiber after being passed through the high-pressure roller is 62%.

[0104] The drying is performed by steam drying, the drying steam pressure is 0.55 MPa, the temperature is 108° C., and the drying time is 32 min.

[0105] The colored cellulose fiber prepared by this method has good color fastness, and the color depth and glossiness are greatly improved compared with the single solution-dyed cellulose fiber. The black cellulose fiber has a color fastness to soaping of 5.0, a color fastness to rubbing of 5.0, a color depth F / S value of 31.362, and a glossiness of 23.61%, which are 7.16% and 8.92% higher than the solution-dyed cellulose fiber prepared with the same amount of black pigment added, respectively.

[0106] Embodiment 3:

[0107] A method for improving the color depth and glossiness of black cellulose fibers, mainly comprising the following steps:

[0108] 1. Preparation of carbon nanotube dispersion system

[0109] Preparation of carbon nanotube dispersion system: Weigh a certain amount of carbon nanotubes and add them into the black color paste (mass fraction of black pigment is 20%) purchased from Suzhou Shiming Technology Co., Ltd., and perform ultrasonic dispersion at room temperature with an ultrasonic frequency of 2×10 9 Hz, treatment time 25min, to obtain a carbon nanotube dispersion system.

[0110] The mass ratio of the carbon nanotubes to the black pigment is 1:20;

[0111] The carbon nanotubes have a purity of 60%, a length of 1 to 3 micrometers, and an outer diameter of 2 to 4 nm.

[0112] 2. Preparation of mixed black slurry dispersion system

[0113] The carbon nanotube dispersion system prepared above was mixed with the black color paste slurry (black pigment mass fraction of 20%) produced by Suzhou Shiming Technology Co., Ltd. in a mass ratio of 1:1, and a pore-forming agent was added, and then deionized water was added for dilution to obtain a mixed black slurry dispersion system.

[0114] The total mass fraction of the black pigment and the carbon nanotubes in the mixed black slurry dispersion system is 10%, and the mass fraction of the pore-forming agent is 5%; the pore-forming agent is sodium bicarbonate.

[0115] 3. Preparation of blended spinning solution

[0116] Cellulose pulp is used as raw material, and a cellulose spinning solution is obtained through a subsequent known viscose preparation process. The mixed black slurry dispersion system prepared above is added according to the effective ingredients, which accounts for a certain proportion of the type A cellulose content in the cellulose spinning solution, to prepare a blended spinning solution.

[0117] The cellulose spinning stock solution contains 10.0% cellulose A, 6.0% sodium hydroxide and a viscosity of 60s.

[0118] The mass ratio of the total mass of the black pigment and the carbon nanotubes to the methyl cellulose content in the mixed black slurry dispersion system is 5.0%.

[0119] 4. Spinning and post-processing

[0120] The blended spinning solution is spun by changing the structure of the spinneret hole (using a cross-shaped spinneret hole), and the primary filament bundle is drawn to obtain a formed filament bundle. The obtained filament bundle is cut, evenly laid into a net, deacidified, first washed, desulfurized, second washed, finished with reactive dyes, cationic modified color fixation, third washed, acid washed, and refined in an oil bath, etc., as well as pressed and dried to obtain black cellulose fibers with significantly improved color fastness and glossiness.

[0121] The coagulation bath composition is 110 g / L sulfuric acid, 20 g / L zinc sulfate, 295 g / L sodium sulfate, and the temperature is 45°C.

[0122] The uniform web laying method is to form a web using a web laying liquid, the web laying liquid is water, the temperature is 99.2°C, and the web laying is carried out by agitation using high temperature water. The high temperature web laying allows carbon disulfide to be evaporated as much as possible, and the thickness of the laid cotton layer is 12 mm.

[0123] The deacidification, first water washing, second water washing and third water washing all use deionized water at a temperature of 80° C. The processing time is controlled according to the chain network speed, and the processing time for each process is 2.5 minutes.

[0124] The desulfurization bath material is sodium sulfide, the concentration is 5.0 g / L, the temperature is 75° C., and the desulfurization time is 6 minutes.

[0125] The reactive dye finishing is to finish the cut short fibers in a dye solution containing a black reactive dye at a temperature of 80° C. for 8 minutes;

[0126] The black reactive dye is reactive black BES, purchased from Shandong Hongfu Chemical Co., Ltd.;

[0127] The dye liquor containing black reactive dye has a mass concentration of 5.0% and a pH value of 7.5;

[0128] The cationic modification and color fixation is to treat the cut short fibers in a cationic modification solution for 5 minutes;

[0129] The concentration of the cationic modifier in the cationic modified solution is 50 g / L, and the pH value is 10;

[0130] The cationic modifier is cationic polyacrylamide, purchased from Qingdao Dayin Chemical Co., Ltd.

[0131] The pickling is carried out using a lactic acid solution with a concentration of 10 g / L and a temperature of 40° C. for 2.5 min;

[0132] The temperature of the oil bath was 65° C., the concentration was 4 g / L, the pH was 9.0, and the treatment time was 5 min.

[0133] The moisture content of the fiber after being passed through the high-pressure roller is 70%.

[0134] The drying is performed by steam drying, the drying steam pressure is 0.60 MPa, the temperature is 120° C., and the drying time is 25 min.

[0135] The colored cellulose fiber prepared by this method has good color fastness, and the color depth and glossiness are greatly improved compared with the single solution-dyed cellulose fiber. The black cellulose fiber has a color fastness to soaping of 5.0, a color fastness to rubbing of 5.0, a color depth F / S value of 32.631, and a glossiness of 25.01%, which are 7.51% and 9.27% ​​higher than the solution-dyed cellulose fiber prepared with the same amount of black pigment added, respectively.

[0136] Comparative Example 1:

[0137] On the basis of Example 2, the steps of reactive dye finishing and cationic modification and color fixation are omitted in the refining process, and the other processes are the same.

[0138] The black cellulose fiber prepared by the method has a color fastness to soaping of 5.0, a color fastness to rubbing of 5.0, a color depth F / S value of 29.571, and a glossiness of 21.19%. Compared with Example 2, the color depth and glossiness are reduced.

[0139] Comparative Example 2:

[0140] On the basis of Example 2, the forming process of the cellulose fiber was not adjusted, and spinning was performed using a conventional circular spinneret, and other processes were the same.

[0141] The black cellulose fiber prepared by the method has a color fastness to soaping of 5.0, a color fastness to rubbing of 5.0, a color depth F / S value of 31.005, and a glossiness of 21.85%. Compared with Example 2, the color depth and glossiness have decreased, but the decrease in glossiness is more obvious.

[0142] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for improving the color depth and glossiness of black cellulose fibers, characterized in that: The method includes the preparation of a carbon nanotube dispersion system, the preparation of a mixed black slurry dispersion system, the preparation of a blended spinning solution, spinning and post-treatment; the post-treatment includes reactive dye finishing and cationic modified color fixation; The preparation method of the carbon nanotube dispersion system is to add carbon nanotubes into black color paste slurry and perform ultrasonic dispersion, with the ultrasonic frequency of 7×10 6 ~2×10 9 Hz, treatment time 25-60 min, to obtain a carbon nanotube dispersion system; The mass fraction of black pigment in the black color paste slurry is 18-25%; The mass ratio of the carbon nanotubes to the black pigment is 1: 18-22; The preparation method of the mixed black slurry dispersion system is to mix the carbon nanotube dispersion system and the black color paste slurry in a mass ratio of 1:1, add a pore-forming agent, and then add deionized water for dilution and preparation to obtain a mixed black slurry dispersion system; The total mass fraction of the black pigment and the carbon nanotubes in the mixed black slurry dispersion system is 10%, and the mass fraction of the pore former is 5%; The preparation method of the blended spinning solution is to add a mixed black slurry dispersion system to the spinning solution to obtain the blended spinning solution; the total mass of the black pigment and the carbon nanotubes in the mixed black slurry dispersion system accounts for 3.5% to 5.0% of the mass of the cellulose alpha in the spinning solution; The spinning is carried out by using a conventional circular spinneret, the composition of the coagulation bath is 90-110 g / L sulfuric acid and 280-295 g / L sodium sulfate; or the spinning is carried out by using a special-shaped spinneret, the composition of the coagulation bath is 90-110 g / L sulfuric acid, 15-20 g / L zinc sulfate, and 280-295 g / L sodium sulfate; the special-shaped spinneret is flat or cross-shaped; The post-treatment includes pickling; the pickling is to treat the fiber with a weak acid solution for 2.5-5 minutes, the concentration of the weak acid solution is 6-10 g / L, and the temperature is 40-60° C.; the weak acid is acetic acid or lactic acid.

2. A method for improving the color depth and glossiness of black cellulose fibers according to claim 1, characterized in that: The reactive dye finishing is carried out in a dye liquor containing a black reactive dye at a temperature of 60-80° C. for a processing time of 8-12 min. The dye liquor containing black reactive dye has a mass concentration of 3.0-5.0% and a pH value of 6.5-7.5; The cationic modification and color fixation is carried out in a cationic modification solution for 5 to 10 minutes; The concentration of the cationic modifier in the cationic modified liquid is 30-50 g / L, and the pH value is 8-10; The cationic modifier is one of a GW type cationic modifier, an RC type cationic modifier or a cationic polyacrylamide.

3. A method for improving the color depth and glossiness of black cellulose fibers according to claim 1, characterized in that: The reactive dye finishing is located after the second washing; and the cationic modified color fixation is located before the third washing.